Hydrochloric Acid → (S)-10-[3-(4-Methoxy-butyl)-4-methyl-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene dihydrochloride

HRID 131469Notes

Reaction equation

HRID 131469 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][C@@H:7]1[N:12]([CH3:13])[CH2:11][CH2:10][N:9]([C:14]2[C:23]3[CH:22]=[C:21]([CH3:24])[S:20][C:19]=3[NH:18][C:17]3[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=3[N:15]=2)[CH2:8]1.[ClH:29].CCOCC>C(Cl)Cl>[ClH:29].[ClH:29].[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][C@@H:7]1[N:12]([CH3:13])[CH2:11][CH2:10][N:9]([C:14]2[C:23]3[CH:22]=[C:21]([CH3:24])[S:20][C:19]=3[NH:18][C:17]3[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=3[N:15]=2)[CH2:8]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 136090333(S)-10-[3-(4-methoxybutyl)-4-methyl-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene

Product 1

HCID 136388584(S)-10-[3-(4-Methoxy-butyl)-4-methyl-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene dihydrochloride

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Into a room temperature stirred solution of (S)-10-[3-(4-methoxybutyl)-4-methyl-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene (0.015 g, 0.038 mmol) in CH2Cl2 add 2.0 N HCl in Et2O (0.038 mL, 0.07 mmol) and stir for 1 h. Concentrate the mixture under reduced pressure and dry in a vacuum oven at 60° C. overnight to give the title compound: brown solid (0.018 g), mass spectrum (m/e):399.0 (M+1).

Workup

  1. concentrationConcentrate the mixture under reduced pressure
  2. customdry in a vacuum oven at 60° C. overnight

Sources & evidence

ORD record
ord-600bbae5a91d4ac1a760b71387b7827d
Source dataset
uspto-grants-2008_06
Patent number
US07384934B2

Reaction notes

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